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Journal of Analytical Chemistry

, Volume 74, Issue 6, pp 574–583 | Cite as

A New Method for Purifying Fat-Containing Extracts in the Determination of Polybrominated Diphenyl Ethers

  • A. A. ShelepchikovEmail author
  • V. V. Ovcharenko
  • A. I. Kozhushkevich
  • E. S. Brodskii
  • A. A. Komarov
  • K. A. Turbabina
  • A. M. Kalantaenko
ARTICLES
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Abstract

We developed a sample preparation method for the determination of polybrominated diphenyl ethers (PBDEs) with from one to ten bromine atoms in samples of feed and food products containing approximately 0.5 g of animal fat or vegetable oil. The method involves gas chromatography with high-resolution mass spectrometry or tandem mass spectrometry. A possibility of using various reagents for the purification of extracts by chemical reactions and fractionation is studied. The physicochemical properties of PBDEs and polychlorinated biphenyls (PCBs) have significant differences, and to determine the full range of PBDEs, it is necessary to use other methods of sample preparation than in the case of PCBs. The conditions selected for the purification of extracts in a column filled with potassium silicate, Florisil, and silica impregnated with sulfuric acid and for their fractionation using activated neutral alumina ensure the PBDE recoveries of at least 75%. Purification of the extracts can be carried out without the use of chlorinated organic solvents. Applied aspects of instrumental analysis and measurement quality assurance are also described.

Keywords:

polybrominated diphenyl ethers sample preparation fractionation food and feed biological samples organic pollutants 

Notes

ACKNOWLEDGMENTS

The authors are grateful to the Center for Ecosystem Safety at the Department of Biology of the Moscow State University for technical support.

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Copyright information

© Pleiades Publishing, Ltd. 2019

Authors and Affiliations

  • A. A. Shelepchikov
    • 1
    • 2
    Email author
  • V. V. Ovcharenko
    • 1
  • A. I. Kozhushkevich
    • 1
  • E. S. Brodskii
    • 2
  • A. A. Komarov
    • 1
  • K. A. Turbabina
    • 1
  • A. M. Kalantaenko
    • 1
  1. 1.The Russian State Center for Animal Feed and Drug Standartization and QualityMoscowRussia
  2. 2.Severtsov Institute of Ecology and Evolution, Russian Academy of SciencesMoscowRussia

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